CN116356403A - Copper foil surface oxidation treatment method - Google Patents

Copper foil surface oxidation treatment method Download PDF

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Publication number
CN116356403A
CN116356403A CN202310234742.XA CN202310234742A CN116356403A CN 116356403 A CN116356403 A CN 116356403A CN 202310234742 A CN202310234742 A CN 202310234742A CN 116356403 A CN116356403 A CN 116356403A
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Prior art keywords
copper foil
anodic oxidation
oxidation treatment
surface oxidation
copper
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陆龙生
雷江
谢颖熙
李凯凯
梅小康
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South China University of Technology SCUT
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    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
    • C25D11/02—Anodisation
    • C25D11/34—Anodisation of metals or alloys not provided for in groups C25D11/04 - C25D11/32
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D7/00—Electroplating characterised by the article coated
    • C25D7/06—Wires; Strips; Foils
    • C25D7/0614—Strips or foils
    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
    • H05K3/00—Apparatus or processes for manufacturing printed circuits
    • H05K3/38—Improvement of the adhesion between the insulating substrate and the metal
    • H05K3/382—Improvement of the adhesion between the insulating substrate and the metal by special treatment of the metal
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10—Energy storage using batteries

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Microelectronics & Electronic Packaging (AREA)
  • Manufacturing Of Printed Wiring (AREA)

Abstract

The invention discloses a copper foil surface oxidation treatment method, which comprises the following steps: immersing copper foil serving as an anode and a platinum sheet serving as a cathode into an anodic oxidation liquid, and then electrifying direct current to carry out anodic oxidation to obtain oxidized copper foil; the anodic oxidation liquid comprises the following components: sodium hydroxide: 3mol/L to 12mol/L; sodium potassium tartrate: 0.1mol/L to 1mol/L; aminocarboxylic acids or/and aminocarboxylates: 0.1mol/L to 0.5mol/L; copper salts: 0.01mol/L to 0.1mol/L; the solvent is water. According to the surface oxidation treatment method of the copper foil, a layer of copper hydroxide film with nano holes is constructed on the surface of the copper foil through anodic oxidation, the peeling strength of the copper foil is improved under the combined action of physical anchoring and chemical anchoring, the interlayer bonding firmness of the manufactured multi-layer board is ensured, meanwhile, the roughness of the copper foil is reduced, and the integrity of signal transmission is improved.

Description

Copper foil surface oxidation treatment method
Technical Field
The invention relates to the technical field of copper foil surface treatment, in particular to a copper foil surface oxidation treatment method.
Background
Along with the continuous deepening of the integration and miniaturization degree of equipment, the printed circuit board gradually develops from a single layer board and a double layer board to a multi-layer board, and the base material of the printed circuit board also develops into a material with lead-free compatibility. Most of matrix resins in the lead-free base material are of aromatic structures, so that the interlayer bonding force of the multilayer board is relatively small, and the bonding condition between layers determines whether the printed circuit board can work normally or not and the performance of the printed circuit board is good or bad. At present, the surface treatment is mainly carried out on the copper foil adhered on the surface of the lead-free substrate, so that the roughness of the surface of the copper foil is increased, and the interlayer bonding strength of the multilayer board is improved. However, with the rapid development of the 5G communication technology, the signal transmission frequency is continuously increased, the communication technology is developed from low frequency and low speed to high frequency and high speed, and in order to ensure the integrity of the high frequency signal transmission to meet the application requirement of high frequency and high speed, the roughness of the copper foil surface needs to be reduced to reduce the conductor loss, so as to reduce the transmission loss of the high frequency signal.
Therefore, it is of great importance to develop a copper foil surface treatment method which can improve both interlayer bonding strength of a multilayer board and signal transmission integrity.
Disclosure of Invention
The invention aims to provide a copper foil surface oxidation treatment method.
The technical scheme adopted by the invention is as follows:
the surface oxidation treatment method of the copper foil comprises the following steps: immersing copper foil serving as an anode and a platinum sheet serving as a cathode into an anodic oxidation liquid, and then electrifying direct current to carry out anodic oxidation to obtain oxidized copper foil; the anodic oxidation liquid comprises the following components: sodium hydroxide: 3mol/L to 12mol/L; sodium potassium tartrate: 0.1mol/L to 1mol/L; aminocarboxylic acids or/and aminocarboxylates: 0.1mol/L to 0.5mol/L; copper salts: 0.01mol/L to 0.1mol/L; the solvent is water.
Preferably, the copper foil is subjected to pickling, degreasing and ultrasonic cleaning.
Preferably, the pickling solution used for pickling is hydrochloric acid.
Preferably, the degreasing liquid used for degreasing is a mixed solution of sodium hydroxide and sodium carbonate.
Preferably, the area ratio of the copper foil to the platinum sheet is 1:0.8-1.2.
Further preferably, the area ratio of the copper foil to the platinum sheet is 1:1.
Preferably, the anodic oxidation liquid comprises the following components: sodium hydroxide: 6mol/L to 8mol/L; sodium potassium tartrate: 0.2mol/L to 0.4mol/L; aminocarboxylic acids or/and aminocarboxylates: 0.1mol/L to 0.2mol/L; copper salts: 0.02mol/L to 0.03mol/L; the solvent is water.
Preferably, the amino carboxylic acid is at least one of 1, 2-diaminocyclohexane tetraacetic acid, ethylenediamine tetraacetic acid and ethylene glycol diethyl ether diamine tetraacetic acid.
Preferably, the amino carboxylate is at least one of trisodium nitrilotriacetate, pentasodium diethylenetriamine pentaacetate and disodium ethylenediamine tetraacetate.
Preferably, the copper salt is copper sulfate.
Preferably, the anodic oxidation is carried out at a current density of 8mA/cm 2 ～20mA/cm 2 Is carried out under the condition of (2).
Further preferably, the anodic oxidation is carried out at a current density of 9mA/cm 2 ～15mA/cm 2 Is carried out under the condition of (2).
Preferably, the anodic oxidation is carried out at the temperature of 25-40 ℃ for 1-10 min.
Further preferably, the anodic oxidation is carried out at a temperature of 25 to 30 ℃ for 1 to 5 minutes.
Preferably, the copper foil is further subjected to water washing and drying after the anodic oxidation is finished.
Preferably, the drying is carried out at a temperature of 90-110 ℃ for 2-5 min.
A copper foil is prepared by the surface oxidation treatment method of the copper foil.
A printed circuit board comprising the copper foil.
The beneficial effects of the invention are as follows: according to the surface oxidation treatment method of the copper foil, a layer of copper hydroxide film with nano holes is constructed on the surface of the copper foil through anodic oxidation, the peeling strength of the copper foil is improved under the combined action of physical anchoring and chemical anchoring, the interlayer bonding firmness of the manufactured multi-layer board is ensured, meanwhile, the roughness of the copper foil is reduced, and the integrity of signal transmission is improved.
Drawings
Fig. 1 is an SEM image of the copper foil in example 1.
Fig. 2 is an SEM image of the oxidized copper foil in example 1.
Detailed Description
The invention is further illustrated and described below in connection with specific examples.
Example 1:
a method for surface oxidation treatment of copper foil, comprising the steps of:
1) Preparing an anodic oxidation liquid: dissolving sodium hydroxide, potassium sodium tartrate tetrahydrate, diethylenetriamine pentasodium pentaacetate and copper sulfate pentahydrate in deionized water to prepare an anodic oxidation solution with the concentration of sodium hydroxide of 7.5mol/L, the concentration of potassium sodium tartrate of 0.3mol/L, the concentration of diethylenetriamine pentasodium pentaacetate of 0.15mol/L and the concentration of copper sulfate of 0.02 mol/L;
2) Anodic oxidation of copper foil: cleaning a copper foil with hydrochloric acid with the mass fraction of 20%, degreasing with degreasing liquid with the sodium hydroxide concentration of 40g/mol and the sodium carbonate concentration of 30g/mol, ultrasonically cleaning with deionized water, immersing the copper foil serving as an anode and a platinum sheet serving as a cathode into an anodic oxidation liquid, wherein the area ratio of the copper foil to the platinum sheet is 1:1, and then supplying direct current and controlling the current density to be 15mA/cm 2 Anodic oxidation is carried out for 2min at 28 ℃, then the copper foil is taken out and washed by deionized water, and then the copper foil is dried for 3min at 100 ℃ to obtain the oxidized copper foil.
A Scanning Electron Microscope (SEM) image of the copper foil in this example is shown in fig. 1, and a SEM image of the oxidized copper foil is shown in fig. 2.
As can be seen from fig. 1 and 2: after the copper foil is subjected to surface oxidation treatment, a copper hydroxide film layer with nano holes is formed on the surface, and the surface roughness is reduced.
Example 2:
a method for surface oxidation treatment of copper foil, comprising the steps of:
1) Preparing an anodic oxidation liquid: dissolving sodium hydroxide, potassium sodium tartrate tetrahydrate, ethylenediamine tetraacetic acid and copper sulfate pentahydrate in deionized water to prepare an anodic oxidation solution with the concentration of sodium hydroxide of 7.5mol/L, the concentration of potassium sodium tartrate of 0.25mol/L, the concentration of ethylenediamine tetraacetic acid of 0.1mol/L and the concentration of copper sulfate of 0.02 mol/L;
2) Anodic oxidation of copper foil: cleaning a copper foil with hydrochloric acid with the mass fraction of 20%, degreasing with degreasing liquid with the sodium hydroxide concentration of 40g/mol and the sodium carbonate concentration of 30g/mol, ultrasonically cleaning with deionized water, immersing the copper foil serving as an anode and a platinum sheet serving as a cathode into an anodic oxidation liquid, wherein the area ratio of the copper foil to the platinum sheet is 1:1, and then supplying direct current and controlling the current density to be 15mA/cm 2 Anodic oxidation is carried out for 4min at 30 ℃, then the copper foil is taken out and washed by deionized water, and then the copper foil is dried for 3min at 100 ℃ to obtain the oxidized copper foil.
Example 3:
a method for surface oxidation treatment of copper foil, comprising the steps of:
1) Preparing an anodic oxidation liquid: dissolving sodium hydroxide, potassium sodium tartrate tetrahydrate, trisodium nitrilotriacetate and copper sulfate pentahydrate in deionized water to prepare an anodic oxidation solution with the concentration of sodium hydroxide of 7.5mol/L, the concentration of potassium sodium tartrate of 0.285mol/L, the concentration of trisodium nitrilotriacetate of 0.156mol/L and the concentration of copper sulfate of 0.03mol/L;
2) Anodic oxidation of copper foil: cleaning a copper foil with hydrochloric acid with the mass fraction of 20%, degreasing with degreasing liquid with the sodium hydroxide concentration of 40g/mol and the sodium carbonate concentration of 30g/mol, ultrasonically cleaning with deionized water, immersing the copper foil serving as an anode and a platinum sheet serving as a cathode into an anodic oxidation liquid, wherein the area ratio of the copper foil to the platinum sheet is 1:1, and then, supplying direct current and controlling the current density to be 9mA/cm 2 Anodic oxidation is carried out for 2min at 25 ℃, and then the copper foil is taken outWashing with deionized water, and drying at 100deg.C for 3min to obtain oxidized copper foil.
Example 4:
a method for surface oxidation treatment of copper foil, comprising the steps of:
1) Preparing an anodic oxidation liquid: dissolving sodium hydroxide, potassium sodium tartrate tetrahydrate, diethylenetriamine pentasodium pentaacetate and copper sulfate pentahydrate in deionized water to prepare an anodic oxidation solution with the concentration of sodium hydroxide of 7mol/L, the concentration of potassium sodium tartrate of 0.4mol/L, the concentration of diethylenetriamine pentasodium pentaacetate of 0.2mol/L and the concentration of copper sulfate of 0.02 mol/L;
2) Anodic oxidation of copper foil: cleaning a copper foil with hydrochloric acid with the mass fraction of 20%, degreasing with degreasing liquid with the sodium hydroxide concentration of 40g/mol and the sodium carbonate concentration of 30g/mol, ultrasonically cleaning with deionized water, immersing the copper foil serving as an anode and a platinum sheet serving as a cathode into an anodic oxidation liquid, wherein the area ratio of the copper foil to the platinum sheet is 1:1, and then supplying direct current and controlling the current density to be 15mA/cm 2 Anodic oxidation is carried out for 1min at 25 ℃, then the copper foil is taken out and washed by deionized water, and then the copper foil is dried for 3min at 100 ℃ to obtain the oxidized copper foil.
Example 5:
a method for surface oxidation treatment of copper foil, comprising the steps of:
1) Preparing an anodic oxidation liquid: dissolving sodium hydroxide, potassium sodium tartrate tetrahydrate, trisodium nitrilotriacetate and copper sulfate pentahydrate in deionized water to prepare an anodic oxidation solution with the concentration of sodium hydroxide of 6mol/L, the concentration of potassium sodium tartrate of 0.3mol/L, the concentration of trisodium nitrilotriacetate of 0.15mol/L and the concentration of copper sulfate of 0.02 mol/L;
2) Anodic oxidation of copper foil: cleaning a copper foil with hydrochloric acid with the mass fraction of 20%, degreasing with degreasing liquid with the sodium hydroxide concentration of 40g/mol and the sodium carbonate concentration of 30g/mol, ultrasonically cleaning with deionized water, immersing the copper foil serving as an anode and a platinum sheet serving as a cathode into an anodic oxidation liquid, wherein the area ratio of the copper foil to the platinum sheet is 1:1, and then supplying direct current and controlling the current density to be 12mA/cm 2 Anode at 28 deg.c for 3minAnd (3) oxidizing, taking out the copper foil, washing with deionized water, and drying at 100 ℃ for 3min to obtain the oxidized copper foil.
Example 6:
a method for surface oxidation treatment of copper foil, comprising the steps of:
1) Preparing an anodic oxidation liquid: dissolving sodium hydroxide, potassium sodium tartrate tetrahydrate, 1, 2-diaminocyclohexane tetraacetic acid and copper sulfate pentahydrate in deionized water to prepare an anodic oxidation solution with the concentration of sodium hydroxide of 6mol/L, the concentration of potassium sodium tartrate of 0.4mol/L, the concentration of 1, 2-diaminocyclohexane tetraacetic acid of 0.15mol/L and the concentration of copper sulfate of 0.02 mol/L;
2) Anodic oxidation of copper foil: cleaning a copper foil with hydrochloric acid with the mass fraction of 20%, degreasing with degreasing liquid with the sodium hydroxide concentration of 40g/mol and the sodium carbonate concentration of 30g/mol, ultrasonically cleaning with deionized water, immersing the copper foil serving as an anode and a platinum sheet serving as a cathode into an anodic oxidation liquid, wherein the area ratio of the copper foil to the platinum sheet is 1:1, and then supplying direct current and controlling the current density to be 15mA/cm 2 Anodic oxidation is carried out for 3min at 28 ℃, then the copper foil is taken out and washed by deionized water, and then the copper foil is dried for 3min at 100 ℃ to obtain the oxidized copper foil.
Comparative example 1:
a method for treating the surface of a copper foil, comprising the steps of:
cleaning the copper foil with 20% hydrochloric acid by mass fraction, degreasing with a degreasing liquid with sodium hydroxide concentration of 40g/mol and sodium carbonate concentration of 30g/mol, ultrasonically cleaning with deionized water, soaking the copper foil in a browning liquid medicine MT (Toguan City, uygur chemical Co., ltd.) for 50s, taking out the copper foil, washing with deionized water, and drying at 100 ℃ for 3min to obtain the surface-treated copper foil.
Comparative example 2:
a method for treating the surface of a copper foil, comprising the steps of:
cleaning the copper foil with 20% hydrochloric acid by mass fraction, degreasing with a degreasing liquid with sodium hydroxide concentration of 40g/mol and sodium carbonate concentration of 30g/mol, ultrasonically cleaning with deionized water, soaking the copper foil in a browning liquid medicine MT (Toguan City, uygur chemical Co., ltd.) for 60s, taking out the copper foil, washing with deionized water, and drying at 100 ℃ for 3min to obtain the surface-treated copper foil.
Comparative example 3:
a method for treating the surface of a copper foil, comprising the steps of:
cleaning the copper foil with 20% hydrochloric acid by mass fraction, degreasing with a degreasing liquid with sodium hydroxide concentration of 40g/mol and sodium carbonate concentration of 30g/mol, ultrasonically cleaning with deionized water, soaking the copper foil in brown chemical liquid HF (An Meite (China chemical Co., ltd.) for 50s, taking out the copper foil, washing with deionized water, and drying at 100 ℃ for 3min to obtain the surface-treated copper foil.
Comparative example 4:
a method for treating the surface of a copper foil, comprising the steps of:
cleaning the copper foil with 20% hydrochloric acid by mass fraction, degreasing with a degreasing liquid with sodium hydroxide concentration of 40g/mol and sodium carbonate concentration of 30g/mol, ultrasonically cleaning with deionized water, soaking the copper foil in brown chemical liquid HF (An Meite (China chemical Co., ltd.) for 60s, taking out the copper foil, washing with deionized water, and drying at 100 ℃ for 3min to obtain the surface-treated copper foil.
Comparative example 5:
copper foil (without surface treatment).
Performance test:
1) The oxidized copper foils of examples 1 to 6 and the surface-treated copper foils of comparative examples 1 to 4 were laminated with prepregs and copper-clad substrates, respectively, and peel strength test samples were prepared and peel strength test was performed with reference to "IPC-TM-650.4.8 peel strength test", and the peel strength test results obtained are shown in the following table:
TABLE 1 peel strength test results
Test item Peel strength (N/mm)
Example 1 0.871
Example 2 0.865
Example 3 0.827
Example 4 0.973
Example 5 0.893
Example 6 0.931
Comparative example 1 0.713
Comparative example 2 0.726
Comparative example 3 0.613
Comparative example 4 0.642
As can be seen from table 1: the surface oxidation treatment method can obviously improve the peeling strength of the copper foil, has better improving effect than the method of browning by adopting two browning liquid medicines in the comparative example, and can well meet the production and use requirements.
2) The surface roughness test was performed on the oxidized copper foils in examples 1 to 6, the surface treated copper foils in comparative examples 1 to 4, and the copper foil in comparative example 5 using a 3D optical profiler (RTEC UP Dual Model), and the obtained surface roughness test results are shown in the following table:
table 2 surface roughness test results
Figure BDA0004121674570000061
Figure BDA0004121674570000071
As can be seen from table 2: compared with the method for browning by adopting two browning liquid medicines in the comparative example, the surface oxidation treatment method provided by the invention has the advantages that the peel strength of the copper foil is improved, the surface roughness of the copper foil is lower, the influence of surface treatment on the loss of transmission signals is reduced, and the integrity of signal transmission is ensured.
The above examples are preferred embodiments of the present invention, but the embodiments of the present invention are not limited to the above examples, and any other changes, modifications, substitutions, combinations, and simplifications that do not depart from the spirit and principle of the present invention should be made in the equivalent manner, and the embodiments are included in the protection scope of the present invention.

Claims (10)

1. The surface oxidation treatment method of the copper foil is characterized by comprising the following steps of: immersing copper foil serving as an anode and a platinum sheet serving as a cathode into an anodic oxidation liquid, and then electrifying direct current to carry out anodic oxidation to obtain oxidized copper foil; the anodic oxidation liquid comprises the following components: sodium hydroxide: 3mol/L to 12mol/L; sodium potassium tartrate: 0.1mol/L to 1mol/L; aminocarboxylic acids or/and aminocarboxylates: 0.1mol/L to 0.5mol/L; copper salts: 0.01mol/L to 0.1mol/L; the solvent is water.
2. The method for surface oxidation treatment of copper foil according to claim 1, wherein: the copper foil is subjected to pickling, degreasing and ultrasonic cleaning.
3. The method for surface oxidation treatment of copper foil according to claim 2, wherein: the pickling solution adopted in the pickling is hydrochloric acid; the degreasing liquid adopted in degreasing is a mixed solution of sodium hydroxide and sodium carbonate.
4. The method for surface oxidation treatment of copper foil according to any one of claims 1 to 3, wherein: the area ratio of the copper foil to the platinum sheet is 1:0.8-1.2.
5. The method for surface oxidation treatment of copper foil according to any one of claims 1 to 3, wherein: the amino carboxylic acid is at least one of 1, 2-diaminocyclohexane tetraacetic acid, ethylenediamine tetraacetic acid and ethylene glycol diethyl ether diamine tetraacetic acid; the amino carboxylate is at least one of trisodium nitrilotriacetate, pentasodium diethylenetriamine pentaacetate and disodium ethylenediamine tetraacetate.
6. The method for surface oxidation treatment of copper foil according to any one of claims 1 to 3, wherein: the anodic oxidation is carried out at a current density of 8mA/cm 2 ～20mA/cm 2 Is carried out under the condition of (2).
7. The method for surface oxidation treatment of copper foil according to any one of claims 1 to 3, wherein: the anodic oxidation is carried out at the temperature of 25-40 ℃ for 1-10 min.
8. The method for surface oxidation treatment of copper foil according to any one of claims 1 to 3, wherein: and after the anodic oxidation is finished, washing and drying the copper foil.
9. A copper foil characterized by being produced by the copper foil surface oxidation treatment method according to any one of claims 1 to 8.
10. A printed circuit board comprising the copper foil of claim 9.
CN202310234742.XA 2023-03-10 2023-03-10 Copper foil surface oxidation treatment method Pending CN116356403A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN117638091A (en) * 2023-12-18 2024-03-01 广东盈华电子科技有限公司 Porous copper foil for lithium battery and preparation method and application thereof

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN117638091A (en) * 2023-12-18 2024-03-01 广东盈华电子科技有限公司 Porous copper foil for lithium battery and preparation method and application thereof

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